CN102659538A - Synthesis technology for preparing methylal by virtue of condensation of methyl alcohol and formaldehyde - Google Patents
Synthesis technology for preparing methylal by virtue of condensation of methyl alcohol and formaldehyde Download PDFInfo
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- CN102659538A CN102659538A CN2012101461985A CN201210146198A CN102659538A CN 102659538 A CN102659538 A CN 102659538A CN 2012101461985 A CN2012101461985 A CN 2012101461985A CN 201210146198 A CN201210146198 A CN 201210146198A CN 102659538 A CN102659538 A CN 102659538A
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- methyl alcohol
- methylal
- formaldehyde
- synthesis technique
- formaldehyde condensation
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Abstract
The invention relates to the field of a catalytic technology and in particular relates to a synthesis technology for preparing methylal by virtue of condensation of methyl alcohol and formaldehyde, and the synthesis technology comprises the operation steps of: adding the methyl alcohol into a four-mouth flask provided with a condenser, then adding formalin into the methyl alcohol and mixing; adding a solid iron system super strong acid catalyst into the mixed solution, and then adopting thermostatic waterbath to treat the mixed solution; and finally, stirring the mixed solution for reaction for half an hour until the reaction liquid is red brown. The high-efficiency synthesis technology for preparing the methylal by condensation of the methyl alcohol and the formaldehyde can be used for remarkably improving the synthesis yield of the methylal, so that the aim of reducing the production cost of the technology can be achieved.
Description
Technical field
The present invention relates to catalysis technical field, the synthesis technique of especially a kind of methyl alcohol efficiently and formaldehyde condensation system methylal.
Background technology
Methylal is Methylal(dimethoxymethane) again, is mainly used in oxidation style production high purity formaldehyde, and the preparation of high purity formaldehyde is the committed step of the good polyoxymethylene resin of production performance.The also alternative formaldehyde of methylal carries out condensation reaction, like phenol or diphenylamine compound and methylal reaction generation diphenol methane or pentanoic methane compound.In recent years, along with the continuous development of the method for making of methylal and utilisation technology and perfect, its purposes has obtained extensive expansion, also makes the methylal product more receive the attention of academia and industry member, and is expected to play a role at the energy and two fields of environment.Along with society is increasingly high to environmental protection requirement, also increasing in the industry for the demand of novel dissolvent and low contaminating chemicals, and methylal is also all the more active as a kind of applied research of novel environment friendly solvent.Methylal is widely used in the products such as automotive industry articles for use, sterilant, leather polish, air freshener, cleaning agent for electronics equipments, colored ribbon, rubber item, paint, makeup, medicine, printing ink.
At present; The production technology enterprise of the high-purity methylal of domestic grasp select quality is considerably less, this just to a great extent limit the exploitation in its field, downstream, and along with the continuous development of national Coal Chemical Industry; The supply of Coal Chemical Industry product strengthens day by day; The consequent is directed to superfluous methyl alcohol and how digests, and occurs a new difficult problem, and the Downstream Products of Methanol of developing energetically will be the focus of for some time from now on.Therefore; With formalin, methyl alcohol is that raw material carries out condensation reaction; Utilize novel reaction rectification technique to produce methylal, work out one cost is low, yield is high, the operational path of good product quality and suitable reactive distillation column internals and its industriallization just seemed be even more important.The catalyzer of the synthesis technique original adoption of methyl alcohol and formaldehyde condensation system methylal is a sulfuric acid; Along with going deep into to catalyst research; Methylal industry synthetic catalyst progressively adopts strong-acid ion exchange resin; We find that the methylal yield of strong-acid ion exchange resin catalysis synthesizing dimethoxym ethane is lower, and this is unfavorable for the energy-saving and emission-reduction transformation of this technology.
Summary of the invention
The technical problem that the present invention will solve is: for overcoming the problem of above-mentioned existence, the synthesis technique of a kind of methyl alcohol efficiently and formaldehyde condensation system methylal is provided, improves the methylal synthesis yield, thereby finally reduce the production cost of this technology.
The technical solution adopted for the present invention to solve the technical problems is: the synthesis technique of a kind of methyl alcohol and formaldehyde condensation system methylal is characterized in that operation steps is following:
A. in the four-hole boiling flask of condensing surface is housed, adding Superlysoform again behind the adding methyl alcohol mixes;
B. add iron in the mixed solution and be behind the solid super acid catalyst through water bath with thermostatic control, the temperature of its water bath with thermostatic control is 39 ℃～43 ℃.
C. be sorrel with mixing solutions stirring reaction half a hour to reaction solution.
Further, in order to reach best methylal yield, the mass ratio of described methyl alcohol and Superlysoform is 16: 9.
Further, described iron is that solid super acid catalyst is made up of the mixture of ferric sulfate and red stone, and the mass ratio of its ferric sulfate and red stone is 2.838, and iron is that solid super acid catalyst can effectively improve speed of reaction.
Further, be 41.8 ℃ through the temperature that experiment showed, the water bath with thermostatic control that it is best, under this temperature, the formaldehyde recovery is the highest.
Its reaction equation is:
The invention has the beneficial effects as follows; The synthesis technique operation steps of a kind of methyl alcohol efficiently of the present invention and formaldehyde condensation system methylal is simple; Can significantly improve the synthesis yield of methylal, thereby reach the purpose of the production cost that reduces this technology, because its cost is low, yield is high, good product quality; Relatively meet the demand of the marketization, help industry and change into product.
Embodiment
Now the present invention is done further detailed explanation.
The synthesis technique concrete steps of a kind of methyl alcohol of the present invention and formaldehyde condensation system methylal are following:
At first, in the 250ml four-hole boiling flask of condensing surface is housed, add 80g methyl alcohol, add 45g Superlysoform then; Wherein, the effect of adopting condensing surface is an expellant gas during methyl alcohol and formolite reaction, is condensed into liquid through heat radiation.
Secondly, in order to improve speed of reaction further, the iron that in the mixing solutions of methyl alcohol and Superlysoform, adds the 3g prepared fresh is solid super acid catalyst;
Once more, under atmospheric pressure state, through water bath with thermostatic control, the scope of this water bath with thermostatic control temperature is 39 ℃～43 ℃ with mixed solution, and its optimum temps is 41.8 ℃, and under this temperature, the formaldehyde yield can reach 100%.Because catalyzer is that sorrel is pulverous, after half a hour, reaction solution is sorrel through stirring reaction.
At last, from reaction solution, extract methylal through distillation technology.
Wherein, iron is that solid super acid catalyst is made up of the mixture of ferric sulfate and red stone, and the mass ratio of this ferric sulfate and red stone is 2.838.Through the experiment proof; Along with iron is the increase of the add-on of solid super acid catalyst; Methylal output also has obvious lifting, surpasses 3g but iron is the solid super acid catalyst add-on, and methylal output amplification begins to reduce; Consider economy, be advisable with 3g so iron is the add-on of solid super acid catalyst.
The synthesis technique operating process of methyl alcohol that the present invention adopted and formaldehyde condensation system methylal is easy; Only need to use a spot of catalyzer just can reach the synthesis yield of higher methylal; Greatly reduce cost, improved the service efficiency of raw material, help suitability for industrialized production.
With above-mentioned foundation desirable embodiment of the present invention is enlightenment, and through above-mentioned description, the related work personnel can carry out various change and modification fully in the scope that does not depart from this invention technological thought.The technical scope of this invention is not limited to the content on the specification sheets, must confirm its technical scope according to the claim scope.
Claims (5)
1. the synthesis technique of methyl alcohol and formaldehyde condensation system methylal is characterized in that operation steps is following:
A. in the four-hole boiling flask of condensing surface is housed, adding Superlysoform again behind the adding methyl alcohol mixes;
B. adding iron in the mixed solution is through water bath with thermostatic control behind the solid super acid catalyst;
C. be sorrel with mixing solutions stirring reaction half a hour to reaction solution.
2. the synthesis technique of a kind of methyl alcohol according to claim 1 and formaldehyde condensation system methylal is characterized in that: the mass ratio of described methyl alcohol and Superlysoform is 16: 9.
3. the synthesis technique of a kind of methyl alcohol according to claim 1 and formaldehyde condensation system methylal is characterized in that: described iron is that solid super acid catalyst is made up of the mixture of ferric sulfate and red stone, and the mass ratio of its ferric sulfate and red stone is 2.838.
4. the synthesis technique of a kind of methyl alcohol according to claim 1 and formaldehyde condensation system methylal is characterized in that: the temperature of water bath with thermostatic control is 39 ℃～43 ℃ among the b.
5. the synthesis technique of a kind of methyl alcohol according to claim 4 and formaldehyde condensation system methylal is characterized in that: the temperature of described water bath with thermostatic control is 41.8 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012101461985A CN102659538A (en) | 2012-05-11 | 2012-05-11 | Synthesis technology for preparing methylal by virtue of condensation of methyl alcohol and formaldehyde |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN2012101461985A CN102659538A (en) | 2012-05-11 | 2012-05-11 | Synthesis technology for preparing methylal by virtue of condensation of methyl alcohol and formaldehyde |
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| CN102659538A true CN102659538A (en) | 2012-09-12 |
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| CN2012101461985A Pending CN102659538A (en) | 2012-05-11 | 2012-05-11 | Synthesis technology for preparing methylal by virtue of condensation of methyl alcohol and formaldehyde |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105254478A (en) * | 2015-09-28 | 2016-01-20 | 常州工程职业技术学院 | Production technology for homogeneous catalytic synthesis of methylal |
| CN116082587A (en) * | 2023-01-30 | 2023-05-09 | 常州工程职业技术学院 | Production process of polyacetal copolymer modified by biological ferulic acid side chain |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1002269A (en) * | 1962-02-21 | 1965-08-25 | Wacker Chemie Gmbh | Process for the manufacture of methylal |
| KR20090090134A (en) * | 2008-02-20 | 2009-08-25 | 주식회사 엘지화학 | Method and apparatus for the production of high purity methylal |
| CN102079740A (en) * | 2010-12-07 | 2011-06-01 | 尹华芳 | Method for preparing butyraldehyde glycol acetal |
| CN102320941A (en) * | 2011-07-14 | 2012-01-18 | 河南煤业化工集团研究院有限责任公司 | Method for synthesizing polyformaldehyde dimethyl ether by taking methanol and methanal as raw materials |
-
2012
- 2012-05-11 CN CN2012101461985A patent/CN102659538A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1002269A (en) * | 1962-02-21 | 1965-08-25 | Wacker Chemie Gmbh | Process for the manufacture of methylal |
| KR20090090134A (en) * | 2008-02-20 | 2009-08-25 | 주식회사 엘지화학 | Method and apparatus for the production of high purity methylal |
| CN102079740A (en) * | 2010-12-07 | 2011-06-01 | 尹华芳 | Method for preparing butyraldehyde glycol acetal |
| CN102320941A (en) * | 2011-07-14 | 2012-01-18 | 河南煤业化工集团研究院有限责任公司 | Method for synthesizing polyformaldehyde dimethyl ether by taking methanol and methanal as raw materials |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105254478A (en) * | 2015-09-28 | 2016-01-20 | 常州工程职业技术学院 | Production technology for homogeneous catalytic synthesis of methylal |
| CN116082587A (en) * | 2023-01-30 | 2023-05-09 | 常州工程职业技术学院 | Production process of polyacetal copolymer modified by biological ferulic acid side chain |
| CN116082587B (en) * | 2023-01-30 | 2024-02-09 | 常州工程职业技术学院 | Production process of polyacetal copolymer modified by biological ferulic acid side chain |
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Application publication date: 20120912 |